KR890000347A - Cerium oxide having a new morphological property and a method of manufacturing the same. - Google Patents

Cerium oxide having a new morphological property and a method of manufacturing the same. Download PDF

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KR890000347A
KR890000347A KR1019880007953A KR880007953A KR890000347A KR 890000347 A KR890000347 A KR 890000347A KR 1019880007953 A KR1019880007953 A KR 1019880007953A KR 880007953 A KR880007953 A KR 880007953A KR 890000347 A KR890000347 A KR 890000347A
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cerium oxide
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로레 쟝-뤽르
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마리-끌로드 뒤트릭 로세
롱쁠랑 쉬미
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Abstract

A process for obtaining a ceric oxide. More precisely, a process for increasing and stabilising the specific surface of a ceric oxide at high temperature. <??>The process of the invention, which consists in preparing a ceric oxide by calcining a ceric hydroxide, is characterised in that the ceric hydroxide is subjected to a solvothermal treatment before the calcination operation.

Description

새로운 형태학적 특성을 갖는 산화 제2세륨 및 그 제조방법.Cerium oxide having a new morphological property and a method of manufacturing the same.

제1도는 소성온도에 따르는 산화 제2세륨의 비표면의 변화를 도시한 도면이다.1 is a diagram showing the change of the specific surface of the second cerium oxide in accordance with the firing temperature.

내용 없음No content

Claims (38)

800~900℃ 사이의 온도에서 소성 후 측정된 비표면이 적어도 15m2/g임을 특징으로 하는 산화 제2세륨.Cerium oxide, characterized in that the specific surface measured after firing at a temperature between 800-900 ° C. is at least 15 m 2 / g. 제1항에 있어서, 800℃의 온도에서 소성후 측정된 비표면 20~600m2/g임을 특징으로 하는 산화 제2세륨.The cerium oxide of claim 1, wherein the specific surface is 20 to 600 m 2 / g measured after firing at a temperature of 800 ° C. 제1 또는 2항에 있어서, 800~900℃ 사이의 온도에서 소성후 측정된 공극부피가 적어도 0.1cm3/g임을 특징으로 하는 산화 제2세륨.The cerium oxide of claim 1 or 2, wherein the pore volume measured after firing at a temperature between 800 and 900 ° C. is at least 0.1 cm 3 / g. 제3항에 있어서, 800℃의 온도에서 소성후에 공극부피가 0.15~0.25cm3/g임을 특징으로 하는 산화 제2세륨.The cerium oxide of claim 3, wherein the void volume is 0.15 to 0.25 cm 3 / g after firing at a temperature of 800 ℃. 제1 내지 4항중 어느 한 항에 있어서, 800℃의 온도에서 소성후에 공극의 평균 직경이 20nm(200Å)~30nm(300Å)임을 특징으로 하는 산화 제2세륨.The cerium oxide according to any one of claims 1 to 4, wherein the average diameter of the pores after firing at a temperature of 800 占 폚 is 20 nm (200 kPa) to 30 nm (300 kPa). 제1 또는 2항에 있어서, 350~900℃ 사이의 온도에서 소성후 측정된 비표면이 15~160m2/g임을 특징으로 하는 산화 제2세륨.The cerium oxide according to claim 1 or 2, wherein the specific surface measured after firing at a temperature between 350 and 900 ° C. is 15 to 160 m 2 / g. 제6항에 있어서, 350~900℃ 사이의 온도에서 소성후에 공극부피가 0.35~0.15cm2/g임을 특징으로 하는 산화 제2세륨.7. The cerium oxide of claim 6, wherein the void volume is 0.35 to 0.15 cm 2 / g after firing at a temperature between 350 and 900 ° C. 350~450℃ 사이의 온도에서 소성후 측정된 비표면이 70~160m2/g이고, 800~900℃의 온도에서 이행되면 적어도 15m2/g의 비표면을 보존함을 특징으로 하는 산화 제2세륨.The specific surface measured after firing at a temperature between 350-450 ° C. is 70-160 m 2 / g, and when carried out at a temperature of 800-900 ° C., the second surface is characterized by preserving at least 15 m 2 / g specific surface. cerium. 제8항에 있어서, 800℃의 온도에서 이행되면 20~60m2/g의 비표면을 보존함을 특징으로 하는 산화 제2세륨.9. The cerium oxide of claim 8, wherein the cerium oxide preserves 20 to 60 m 2 / g specific surface when transferred at a temperature of 800 ° C. 제8 또는 9항에 있어서, 350~450℃ 사이의 온도에서 소성된 후 측정된 비표면이 100~160m2/g임을 특징으로 하는 산화 제2세륨.10. Cerium oxide according to claim 8 or 9, characterized in that the specific surface measured after firing at a temperature between 350-450 ° C is 100-160 m 2 / g. 제8 내지 10항중 어느 한 항에 있어서, 350℃의 온도에서 소성후에 공극의 평균 직경이 10mm(100Å)~20nm(200Å)임을 특징으로 하는 산화 제2세륨.The cerium oxide according to any one of claims 8 to 10, wherein the average diameter of the pores after firing at a temperature of 350 ° C is 10 mm (100 mm) to 20 nm (200 mm). -세륨염의 용액과 염기(염기의 비율은 반응 매질의 pH가 7이상이 되게함) 경우에 따라서는 산화제 존재하에 반응시켜 수산화 제2세륨을 제조하고; 수득된 침전물을 분리하고, 경우에 따라서는 그것을 세척하며; -수산화 제2세륨을 물 또는 분해 가능한 염기의 수용액에 현탁시키고; -그것을 밀폐용기내에서 상기 매질의 임계온도 및 임계압력 이하의 온도 및 압력까지 가열하고; -반응 혼합물을 냉각하고 압력을 대기압으로 낮추고; -그렇게 처리된 수산화 제2세륨을 분리하고; -그다음 그것을 소성함으로 구성됨을 특징으로 하는 제1 내지 11항중 어느 한 항에 설명된 산화 제2세륨이 제조방법.A solution of cerium salt and a base (the proportion of the base causes the pH of the reaction medium to be 7 or more) and in some cases reacted in the presence of an oxidizing agent to prepare second cerium hydroxide; The precipitate obtained is separated off and optionally washed; -Cerium hydroxide is suspended in an aqueous solution of water or degradable base; Heating it in a closed container to a temperature and pressure below the critical temperature and the critical pressure of the medium; Cooling the reaction mixture and lowering the pressure to atmospheric pressure; Separating the cerium hydroxide so treated; And then the cerium oxide as described in any one of claims 1 to 11, characterized in that it is composed by firing it. 제12항에 있어서, 세륨염의 용액은 염화 제1세륨의 용액, 제1세륨 또는 제2세륨 상태의 세륨의 니트레이트의 용액, 또는 이들 사이의 혼합물임을 특징으로 하는 산화 제2세륨의 제조방법.13. The method of claim 12, wherein the solution of cerium salt is a solution of cerium chloride, a solution of nitrate of cerium in the first or second cerium state, or a mixture therebetween. 제12항에 있어서, 세륨염의 용액은 질산 제2세륨의 수용액이거나 또는 산화제의 존재하에 사용되는 질산 제1세륨의 수용액임을 특징으로 하는 산화 제2세륨의 제조방법.The method for producing cerium oxide according to claim 12, wherein the solution of cerium salt is an aqueous solution of cerium nitrate or an aqueous solution of cerium nitrate used in the presence of an oxidizing agent. 제14항에 있어서, 세륨염의 용액은 질산 제1세륨을 전기 화학적으로 산화하거나 또는 수화된 산화 제2세륨에 질산을 작용시켜 산출된 질산 제2세륨의 수용액임을 특징으로 하는 산화 제2세륨이 제조방법.15. The preparation of cerium oxide according to claim 14, wherein the solution of cerium salt is an aqueous solution of cerium nitrate produced by electrochemically oxidizing cerium nitrate or by acting nitric acid on a hydrated cerium oxide. Way. 제12 내지 15항중 어느 한 항에 있어서, 염기가 암모니아 용액임을 특징으로 하는 산화 제2세륨의 제조방법.The process for producing cerium oxide according to any one of claims 12 to 15, wherein the base is an ammonia solution. 제14항에 있어서, 산화제가 과산화 수소수임을 특징으로 하는 산화 제2세륨의 제조방법.The method for producing cerium oxide according to claim 14, wherein the oxidant is hydrogen peroxide solution. 제12 내지 17항중 어느 한 항에 있어서, 첨가된 염기의 양은 상기 반응 매질의 pH가 7.0 이상 및 약 10 이하가 되게함을 특징으로 하는 산화 제2세륨의 제조방법.18. The process of any of claims 12-17, wherein the amount of base added causes the pH of the reaction medium to be at least 7.0 and at most about 10. 제18항에 있어서, 상기 pH는 7.5~9.0 사이임을 특징으로 하는 산화 제2세륨의 제조방법.19. The method of claim 18, wherein the pH is between 7.5 and 9.0. 제12 내지 19항중 어느 한 항에 있어서, 반응 매질의 온도가 5~70℃임을 특징으로 하는 산화 제2세륨의 제조방법.20. The process for producing cerium oxide according to any one of claims 12 to 19, wherein the temperature of the reaction medium is 5-70 [deg.] C. 제20항에 있어서, 반응매질의 온도가 40~70℃ 사이임을 특징으로 하는 산화 제2세륨의 제조방법.21. The method of claim 20, wherein the temperature of the reaction medium is between 40 and 70 &lt; 0 &gt; C. 제12 내지 21항중 어느 한 항에 있어서, 분리된 수산화 제2세륨은 물에서 또는 염기성 용액을 사용하여 세척됨을 특징으로 하는 산화 제2세륨의 제조방법.22. The process for producing cerium oxide according to any one of claims 12 to 21, wherein the separated cerium hydroxide is washed in water or using a basic solution. 제12항에 있어서, 수산화 제2세륨이 하기 일반식(I)에 부합함을 특징으로 하는 산화 제2세륨의 제조방법.The process for producing cerium oxide according to claim 12, wherein the cerium hydroxide is in accordance with the following general formula (I). Ce(OH)x(X)y, nH2O (I)Ce (OH) x (X) y , nH 2 O (I) 상기식에서, x는 클로라이드 또는 니트레이트 음이온을 나타내고, y는 0.5 이하이고, x=4-y이고, n은 0~약 20이다.Wherein x represents a chloride or nitrate anion, y is 0.5 or less, x = 4-y and n is 0 to about 20. 제23항에 있어서, 수산화 제2세륨은 식중 y가 0~0.1인 일반식(I)에 부합함을 특징으로 하는 산화 제2세륨의 제조방법.The method for producing cerium oxide according to claim 23, wherein the second cerium hydroxide corresponds to general formula (I) in which y is 0 to 0.1. 제24항에 있어서, 일반식(I)의 수산화 제2세륨은 염화 제1세륨 또는 질산 제1세륨 및 암모니아 용액을 산화제의 존재하에 7.5~9.0 사이의 pH 및 40~70℃ 사이의 온도에서 반응시키고 침전물을 분리하고 그것을 세척하여 제조됨을 특징으로 하는 산화 제2세륨의 제조방법.The method of claim 24, wherein the second cerium hydroxide of formula (I) reacts the first cerium chloride or first cerium nitrate and ammonia solution at a pH between 7.5 and 9.0 and a temperature between 40 and 70 ° C in the presence of an oxidizing agent. And the precipitate is separated and washed to prepare the method of producing cerium oxide. 제12항에 있어서, 분해가능한 염기는 암모니아, 우레아, 탄산수소암모늄, 탄산암모늄, 1급, 2급, 3급 또는 4급아민, 또는 이들의 혼합물임을 특징으로 하는 산화 제2세륨의 제조방법.13. The process of claim 12, wherein the degradable base is ammonia, urea, ammonium bicarbonate, ammonium carbonate, primary, secondary, tertiary or quaternary amine, or mixtures thereof. 제26항에 있어서, 분해 가능한 염기는 암모니아, 테트라알킬 암모늄 히드록시드 또는 이들의 혼합물임을 특징으로 하는 산화 제2세륨의 제조방법.27. The method of claim 26, wherein the degradable base is ammonia, tetraalkyl ammonium hydroxide, or mixtures thereof. 제26 또는 27항에 있어서, 염기성 용액의 농도는 1~10N 사이임을 특징으로 하는 산화 제2세륨의 제조방법.28. The method of claim 26 or 27, wherein the concentration of the basic solution is between 1 and 10 N. 제12 내지 28항중 어느 한 항에 있어서, CeO2로 표시되는 수산화 제2세륨의 농도는 0.3~6몰/l임을 특징으로 하는 산화 제2세륨의 제조방법.29. The method for producing cerium oxide according to any one of claims 12 to 28, wherein the concentration of the second cerium hydroxide represented by CeO 2 is 0.3 to 6 mol / l. 제29항에 있어서, 상기 농도는 2~3몰/l임을 특징으로 하는 산화 제2세륨이 제조방법.30. The method of claim 29, wherein the concentration is 2-3 mol / l. 제12 내지 30항중 어느 한 항에 있어서, 오토클레이브 처리 온도가 100~350℃임을 특징으로 하는 산화 제2세륨의 제조방법.The method for producing cerium oxide according to any one of claims 12 to 30, wherein the autoclave treatment temperature is 100 to 350 ° C. 제31항에 있어서, 상기 온도가 150~350℃임을 특징으로 하는 산화 제2세륨의 제조방법.The method of claim 31, wherein the temperature is 150 ~ 350 ℃. 제12 내지 32항중 어느 한 항에 있어서, 압력은 1바(1×105Pa)~165바(165×105Pa) 임을 특징으로 하는 산화 제2세륨의 제조방법.33. The method of claim 12, wherein the pressure is between 1 bar (1 × 10 5 Pa) and 165 bar (165 × 10 5 Pa). 제33항에 있어서, 상기 압력은 5바(5×155Pa)~165바(165×105Pa) 임을 특징으로 하는 산화 제2세륨의 제조방법.34. The method of claim 33, wherein the pressure is between 5 bar (5 x 15 5 Pa) and 165 bar (165 x 10 5 Pa). 제31 내지 34항중 어느 한 항에 있어서, 오토클레이브 처리시간은 30분~6시간임을 특징으로 하는 산화 제2세륨의 제조방법.35. The method for producing cerium oxide according to any one of claims 31 to 34, wherein the autoclave treatment time is 30 minutes to 6 hours. 제12 내지 35항중 어느 한 항에 있어서, 소성 온도는 300~1000℃임을 특징으로 하는 산화 제2세륨의 제조방법.36. The method for producing cerium oxide according to any one of claims 12 to 35, wherein the firing temperature is 300 to 1000 deg. 제36항에 있어서, 상기 온도가 350~800℃임을 특징으로 하는 산화 제2세륨의 제조방법.37. The method of claim 36, wherein the temperature is 350-800 ° C. 제35 또는 36항에 있어서, 소성 시간이 2~6시간임을 특징으로 하는 산화 제2세륨의 제조방법.37. The method for producing cerium oxide according to claim 35 or 36, wherein the firing time is 2 to 6 hours. ※참고사항 : 최초출원 내용에 의하여 공개하는 것임.※ Note: It is to be disclosed based on the initial application.
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